Apparatus for the production of finely divided substances



Aug.12,-1941.. E. w. SMITH 2,251,959

APPARATUS .FOR EM-IE PRODUCTION OF FINELY DIVIDED SUBSTANCES Original Filed Dec. 27, 1955 6 (Ill/W Flef2' INVENTOR gDWARDWSMITH.

ATTORNEY Patented Aug. 12, 1941 APPARATUS FOR THE PRODUCTION OF FINELY DIVIDED SUBSTANCES Edward W. Smith, Melrose, Mass, assignor to Submarine Signal Company, Boston, Mass, a corporation of Maine Original application December 27!, 1935, Serial No. 56,365. Divided and this application Uctov ber 22, 1938, Serial No. 236,502

2 Claims.

The' present application is a division of application Serial No. 56,365, filed December 27, 1935.

The present invention relates to an apparatus for the manufacture of finely divided materials produced by the reaction of two or more substances, particularly to the production of finely divided substances in the form of precipitates produced by such reaction.

Heretofore in the production of finely divided (bi. 211L193) ratus suitable for the application of vibrational energy to reacting liquids, in a continuously operable system for the production of finely divided precipitates. I

The latter is particularly adaptable to cases where one of the reacting substances is only difiicultly soluble. For example, precipitated calcium carbonate, which is used commercially in the manufacture of tooth pastes, the sizing of paper substances in the form of precipitates it has been and for other purposes is ordinarily obtained customary simply to mix the reacting solutions, commercially as a Icy-product in the manufacture to allow the precipitate which is formed to setof caustic soda. The usual method of procedure tie at the bottom of the reaction chamber and is to fill a large tank with water and add to it' after removing the remaining liquid to wash and lime or calcium oxide and a suitable amount of dry the precipitate. While the precipitate which sodium carbonate. The mixture is then heated. is produced by this method is usually in a finely By lnteraction between the water and the calcium divided state, the division is often. insufiiciently oxide, calcium hydroxide is formed. As fast as fine, making it necessary to use some grinding the latter is produced, it reacts with the sodium process in order to reduce the coarse particles, carbonate until finally the tanlr contains caustic or where this is not possible, the product or proc- 2o soda and a fine white precipitate of calcium caress in which the precipitate is used may not be as bonate. According to the present invention, indesirable as would be the case if a more finely tence vibrational energy is applied to the liquids divided material were available. while the reaction is taking place and more par- On the other hand, in the manufacture of ticularly such vibrational energy is applied at the photographic emulsions, it is desirable to obtain 2: instant and at the point where the two reacting a fine-grained silver halide suspended in a bindl q id f r xamp e. c l i hyd xide n dier, such as gelatin. Here, too, the customary um carbonate, come into contact with each other. practice has-been to produce the silver halide by Fu t er re. th p t invention p d s a the reaction between a silver salt solution, such Syste f r c rrys out this process Without the as silver nitrate, and a halogen salt, such as pouse of excessive amounts of water, in spite of the tassium chloride. The products of this reaction smalls lu oi c Oxideare soluble potassium nitrate and precipitated The above and other features of my invention silver chloride. The gelatin binder is usually. will be understood from the following description mixed with one of the reacting liquids before the taken in c nne i n with th mp ny reaction takes place. Later, the soluble potassidrawin in Which s- 1 Shows a Cross Section Of um nitrate is removed by washing. According to an apparatus r pp y g Vibrational e r y the present invention, extremely fine-grained reacting l qu 2 Shows schematically a 31 photographic emulsions are produced by carrytem for the production of finely divided preclpi ing out the silver halide precipitating reaction tates. only under the influence of intense compressional In Figl e diaphragm is adapted to be Set wave vibration. into intense vibration by the action of the elec- This is accomplished by means of the appatromagnet 2 upon the armature t which is fixed ratus of the present invention which is so arto the diaphragm l. The electromagnet 2 is enranged that the two reacting solutions are ergized by the winding i and is mounted within brought into contact with each other only while a casing b to which the diaphragm is securely each of them is subjected to intense compressionfastened by means of screws t. A bove thedia= a1 wave vibration, 1 which vibration is continued phragm there is mounted a recessed cover plate until the reaction process is completed. l by means of the screws t forming a'thin fiat Apparatus for the treatment of liquids with inreaction chamber ii. The thickness of the chain'- tense compressional wave vibrations has previ ber t is preferably of the order of 0.1 inch. Atously been known in'the art as shown, for examtached to the cover '0 is a smaller plate it which ple, by Patent No. 2,138,051, to Robert L. Wilis provided with an annular groove ll communiliams, issued November 29, 1938. The present ineating with thereaction chamber t through a vention concerns similar apparatus. plurality of holes i t in the cover l.

The present invention also provides an appa- A pipe it serves toconduct one of the reacting liquids into the chamber 9, the other liquid being conducted to the reaction chamber by means of the pipe l4 leading to the groove II and thence through the holes 12. An exit for the liquids is provided by the hole l5 extending through the cover 1 and the plate l0 and communicating with the outlet pipe IS.

The apparatus may be employed in the following manner: One of the reacting liquids, for example, potassium chloride solution is permitted to enter the reaction chamber 9 by means of the pipe I3- after the diaphragm has been seta chemical'reaction producing potassium nitrate and a precipitate of silver chloride. The resulting liquid with the precipitate in suspension then flows out through the pipe IB. Gelatin orother binder may, if desired, be added to one of the reacting liquids before it enters. the reaction chamber.

It will be noted that the apparatus 'just described is so arranged that the two reacting liquids can only come in contact with each other at a point where they are subject to intense compressional wave vibrations. It will also be understood that the rates of flow of the reacting liquids into the reaction chamber are adjusted so that the reaction is complete before the liquid leaves the reaction chamber. Furthermore, it will be evident that if more than two liquids are required to effect the reaction resulting in the formation of the desired precipitate, additional tank 20 where it is available for the solution of aditional lime to provide calcium hydroxide for further action in the vibrator with sodium carbonate. Valves 28 and 29 may be employed to regulate therates of flow of the two solutions.

With the system 'just described itis possible to operate with a relatively small quantity of water since the liquid is used over and over again until the resulting sodium hydroxide becomes so concentrated that it is not able any longer to dissolve appreciable amounts of lime.

In the event that the system is to be used for the production of some other precipitate where perhaps an. excessive amount of water is not required, the pipe 21 may lead to a storage tank or other device instead of to the tank 20 as may appear to be desirable. The system is thus also useful for producing fine-grained photographic emulsions as above described. In this case the filter 26 would, of course-also be omitted. While the present invention has been described above with. particular reference to the production entrances may readily be provided to the reaction chamber.

In some instances, one of the" reacting substances is only difliculty soluble as in the case of the calcium carbonate precipitating reaction mentioned above, where one of the reacting liquids, calcium hydroxide, is'conveniently produced by mixing lime with water. Calcium hydroxide cannot readily be produced in very great concentration in this manner, and'hence' a relatively large amount of water is required to provide enough calcium hydroxide to react with a given volume of sodium carbonate.

Fig. 2 illustrates a complete system for carrying out this process without using undue quantities of water, I the tank 20 and conducted to the vibrator 2| by means of the pipe 22. The sodium carbonate After the reaction under the influence, of compressional wave vibration has been completed, the resulting liquid passes out of the oscillator through the pipe 25 The lime and water are mixed in solutioirn tank 23 is conducted to the oscillator by" means of the pipe 24,

and into the filter 26 where the precipitated calcium carbonate is. separated from the liquid which consists of a solution of sodium hydroxide. This is pumped back through the pipe]? into the of fine-grained photographic emulsions and of precipitated calcium carbonate, it will be evident that it is applicableto the production of other precipitates. Having now described my invention, I claim:

1; Apparatus for the production of finely divided precipitates by the reaction of two substances which comprises a vibratable diaphragm, means for vibrating the same, a recessed cover plate, means for mounting the same over the diaphragm thereby forming a thin, flat chamber having said diaphragm asone wall thereof,

an aperture in said cover plate adapted to con-. duct a reactive substance into said chamber, a group of other apertures in sa id cover leading into said chamber at points spaced away from said first aperture, a plate having an annular groove mounted upon said cover with said groove in pommunication with said group of. other aper tures, means for conducting. the other reactive substance to saidannular groove and means for withdrawing reaction products from said chamber. 2. Apparatus for producing finely divided precipitates by the reaction of two or more liquids comprising'means producing compressional wave vibrations, said means having a substantially plane vibrating surface, means forming a thin, substantially flat enclosed chamber with-one wall thereof comprising said vibrating surface, a plate forming the opposite wall of said chamber'and being positioned substantially parallel and close to said vibrating surface, whereby a space is provided through which liquid can flow, an inlet to said chamber near-the edge'thereof for one of the reacting liquids, separate inlets into said chamber through-said plate and spaced between the center and the edge of the plate for the other reacting liquids and an outlet for the reaction products at the center of the plate.

' EDWARD w. SMITH. 

